Month: April 2021

Related Products of 956317-36-5, The chemical industry reduces the impact on the environment during synthesis 956317-36-5, name is 5-Methyl-2-(2H-1,2,3-triazol-2-yl)benzoic acid, I believe this compound will play a more active role in future production and life.

EXAMPLE B5-Fluoro-2-{r(3R,6R)-l-(2-iodo-5-methylben2oyl)-6-methylpiperidin-3-yllmethoxy}pyridine (B- To a solution of A?7 (325 mg, 1.5 mmol) in CH2CI2 (50 ml) at 0C was added diisopropylethylamine (506 mL, 2.9 mmol) followed by C-I (447 mg, 1.6 mmol, generated from A-8 by treatment with SOCI2 and catalytic DMF in CH2CI2). After warming to room temperature and stirring for 2 h, the reaction was partitioned between CH2CI2 and saturated aqueous NaHC03. The layers were separated, the aqueous was extracted again with CH2CI2, the combined organics were washed with water, dried over Na2SO4, filtered and concentrated. The crude material was purified by gradient elution on silica gel (0 to 100% EtOAc in Hex) to yield 530 mg of B1^aS a white solid. Data for B1^: LRMS m/z (M+H): 469.1.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 5-Methyl-2-(2H-1,2,3-triazol-2-yl)benzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK & CO., INC.; WO2008/147518; (2008); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Some common heterocyclic compound, 288-36-8, name is 1H-1,2,3-Triazole, molecular formula is C2H3N3, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Product Details of 288-36-8

A solution of 2-iodobenzoic acid (3.0 g, 12.09 mmol) in DMF (1.0 mL) was treated with 1,2,3-triazole (1.5 g, 21.7 mmol), CsCO3 (7.08 g, 21.7 mmol), and trans-N,N’- dimethylcyclohexane-l52-diamine (0.31 g, 2.17 mmol). The mixture was heated at 120 0C for 10 min in a microwave reactor. The reaction was cooled to rt, diluted with EtOAc5 and filtered through Celite. The residue was purified by gradient elution on SiO2 (0 to 10% MeOH in DCM with 0.1% AcOH) to give the faster eluting desired 2-(2H-l52,3-triazol-2-yl)benzoyl acid. Data for 2-triazolyl isomer: 1HNMR (500 MHz, DMSO-d6) delta 13.05 (br s , IH)5 8.12 (s, 2H), 7.81-7.52 (m, 4H) ppm. The undesired l-(2H-l,2,3-triazol-2-yl)benzoic acid eluted second. A portion of the desired acid (0.10 g, 0.53 mmol) was treated with thionyl chloride (0.59 g, 5.3 mmol) in dichloromethane (5.0 mL) at rt. After stirring at RT for 1 h, the mixture was concentrated, azeotroping with benzene to yield acid chloride A-3.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 288-36-8, its application will become more common.

Reference:
Patent; MERCK & CO., INC.; WO2007/126934; (2007); A2;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Related Products of 288-88-0, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 288-88-0, name is 1H-1,2,4-Triazole belongs to triazoles compound, it is a common compound, a new synthetic route is introduced below.

EXAMPLE 1 STR56 4.15 g (0.103 mole) of sodium hydroxide and a spatula-tip of azo-bis-isobutyronitrile were added to a solution of 71.55 g (0.3 mole) of 2-tert.-butyl-2-(4-chloro-phenyl-ethyl)-oxirane in 10 ml of N-methylpyrrolidone. The mixture was heated to 120 C. and a solution of 20.7 g (0.3 mole) of 1,2,4-triazole was added dropwise in the course of 3 hours, with stirring. The mixture was then stirred at 120 C. for a further hour and then allowed to cool. Thereafter, it was worked up by a procedure in which the N-methyl-pyrrolidone was distilled off at a bath temperature of 100 C. under a pressure of 0.2 mbar and the residue which remained was washed with water and then dried and stirred with 150 ml of benzine. The solid product which deposited was filtered off and dried again. 78.9 g (85.8% of theory) of 1-(4-chloro-phenyl)-4,4-dimethyl-3-(1,2,4-triazol-1-yl-methyl)-pentan-3-ol were obtained in this manner. It was demonstrated by analysis by HPLC that the product is not contaminated by the corresponding 1,3,4-triazole derivative.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 1H-1,2,4-Triazole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Bayer Aktiengesellschaft; US4626594; (1986); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Some common heterocyclic compound, 41253-21-8, name is Sodium 1,2,4-triazol-1-ide, molecular formula is C2H2N3Na, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Recommanded Product: Sodium 1,2,4-triazol-1-ide

10.0 g of the compound of formula (FF) as oil, as obtained according to Reference Example 1.1.e, were dissolved in 80 ml of DMSO under stirring. Then, 10 g of the sodium salt of 1,2,4-triazole were added at 25 to 30 C., and the resulting reaction mixture was stirred for 24 hours at 85 to 90 C. The mixture was then cooled to 25 to 30 C., and 25 ml of 5% (w/v) aqueous solution of sodium hydroxide were added. The mixture was then stirred for 3 hours at 25 to 30 C. 100 ml of water were added, and the product was extracted into 150 ml of methyl tetrahydrofuran. The thus obtained organic layer was washed with a 10% (w/v) aqueous solution of sodium chloride, and subsequently the solvents of the resulting separated organic layer were removed by distillation under reduced pressure to obtain the title compound of formula (GG) as a crude oil. The yield was 6.0 g, corresponding to a theoretical value of 86.0%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 41253-21-8, its application will become more common.

Reference:
Patent; SANDOZ AG; Wilhelm, Thorsten; Langner, Martin; US2014/303184; (2014); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

These common heterocyclic compound, 1001401-62-2, name is 2-(2H-1,2,3-Triazol-2-yl)benzoic acid, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. SDS of cas: 1001401-62-2

j0814] To the title compound of step B (140 mg, 0.5 mmol) and intermediate A-i (113 g, 0.6 mmol) in DMF (4 mE) was added DIPEA (230 jt, 1.4 mmol) and HATU (155 g, 0.6 mmol). Upon completion of the reaction, purification was performed using Agilent prep method X to give the title compound (172 g, 74%). MS (ESI) mass calcd. for C2QH,8F3N70, 429.2; mlz found 430 [M+H]. 1H NMR (CDC13): 8.32 (s, 0.3H), 8.17 (s, 0.7H), 7.99-7.89 (m, i.5H), 7.88-7.77 (m, 1 .5H), 7.62-7.30 (m, 4H), 6.24-6.15 (m, 0.3H),4.86 (s, 0.7H), 4.76 (d, J=5.4 Hz, 0.3H), 4.45-4.23 (m, 1H),

The synthetic route of 2-(2H-1,2,3-Triazol-2-yl)benzoic acid has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Janssen Pharmaceutica NV; COATE, Heather R.; DVORAK, Curt A.; FITZGERALD, Anne E.; LEBOLD, Terry P.; PREVILLE, Cathy; SHIREMAN, Brock T.; (473 pag.)US2016/46640; (2016); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

6523-49-5, name is 4-(1,2,4-Triazol-1-yl)aniline, belongs to triazoles compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Computed Properties of C8H8N4

To a solution of Intermediate 19 (95mg, 0.29mmol) in acetic acid (ImI) was added A- triazolylaniline (56mg, 0.35mmol) and the solution was stirred at 8O0C over 2 hours. LCMS analysis showed consumption of starting material.Reaction mixture was cooled and the excess acetic acid removed by evaporation under reduced pressure. The residues were treated with sat. aq. Sodium hydrogen carbonate until cessation of effervescence. The resulting precipitate was filtered and the solids obtained dried under vacuum. Purification by preparative chromatography furnished the desired compound as an off- white solid (33mg, 25%)1H NMR (D6-DMSO) 10.24 (IH, bs), 9.27 (IH, s), 8.82 (IH, s), 8.64 (IH, s), 8.36 (IH, s), 8.24 (IH, s), 8.22 (IH, dd, J 9Hz, 1.75Hz), 8.09 (2H, d, J 9Hz), 7.92 (3H, m), 7.64 (IH, dd, J 8.25Hz, 2Hz), 7.46 (IH, m), 4.87 (IH, quin, J 6Hz), 1.36 (6H, d, J 6Hz) LC-MS rt 2.66 m/z 441 ES+

The synthetic route of 6523-49-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ARROW THERAPEUTICS LIMITED; WO2007/80401; (2007); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Some common heterocyclic compound, 41253-21-8, name is Sodium 1,2,4-triazol-1-ide, molecular formula is C2H2N3Na, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. HPLC of Formula: C2H2N3Na

150 g (1 eq) of compound G was added to 1.5 L of DMF and added178 mg (5 eq) of sodium triazole and 38 ml of 1,3-dimethylpropylene urea (DMPU),And the mixture was stirred at 100 to 110 C for 24 hours.The reaction mixture was cooled to room temperature, 1.5 L of water was added to the reaction solution, and impurities were extracted with 400 ml of * 2 DCM. The organic phase was washed with 300 ml of 6NHCl extraction, hydrochloric acid aqueous solution with 100ml * 2DCM washing, separation of hydrochloric acid aqueous solution, temperature control below 30 50% NaOH adjusted PH = 8-9, extracted with 500ml * 2EA, combined EA, 300ml * 5 washing, 300mlBrine, brine, dried over Na2SO4 and concentrated to give a yellow oil. 200 ml of EA was added,Solution, dropping 800ml n-heptane solid wash, stirring at room temperature 3h, suction filtration, 200ml n-heptane washing, wasTo a white solid compound H of 86.9 g, Y = 68.5%, pur = 95.2%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 41253-21-8, its application will become more common.

Reference:
Patent; Chongqing Weipeng Pharmaceutical Co., Ltd; Han, Gongchao; Zhou, Zhiliang; Zhou, Xingguo; Xiang, Yong; Xiang, Linling; Gong, Xue; (8 pag.)CN105440022; (2016); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 16681-70-2, name is 1H-[1,2,3]Triazole-4-carboxylic acid, A new synthetic method of this compound is introduced below., Recommanded Product: 1H-[1,2,3]Triazole-4-carboxylic acid

Example 22 1-Acetyl-3-{(R)-3-(5?-chloro-2?-fluorobiphenyl-4-yl)-2-[(3H-[1,2,3]triazole-4-carbonyl)amino]propyl}pyrrolidine-3-carboxylic Acid (isomers a and b) [0464] 1-Acetyl-3-[(R)-2-amino-3-(5?-chloro-2?-fluorobiphenyl-4-yl)propyl]pyrrolidine-3-carboxylic Acid (isomer a; 10 mg) dissolved in DMF. 1H-1,2,3-triazole-4-carboxylic acid (2 eq.), DIPEA (2 equiv.), and HATU (1 equiv.) were also dissolved in DMF and stirred at room temperature for a few minutes. The solutions were then combined and the resulting mixture stirred at room temperature until the reaction was complete (as seen by LCMS). The mixture was concentrated in vacuo and purified by preparative HPLC to yield the title compound (isomer a; 4.1 mg). LCMS (ESI): calc. C25H25ClFN5O4=513; obs. M+H=514.3. Retention time: 2.24 min. [0466] 1-Acetyl-3-[(R)-2-amino-3-(5?-chloro-2?-fluorobiphenyl-4-yl)propyl]pyrrolidine-3-carboxylic Acid (isomer b; (40 mg, 88 mumol, 1.0 eq.) and DIPEA (50 muL, 170 mumol, 2.0 eq.) were dissolved in DMF (0.2 mL). 1H-1,2,3-triazole-4-carboxylic acid (30 mg, 260 mumol, 3.0 eq.), DIPEA (90 muL, 340 mumol, 4.0 eq.) and HATU (65 mg, 170 mumol, 1.9 eq.), were dissolved in DMF (0.6 mL) and stirred at room temperature for 30 minutes. The solutions were then combined and the resulting mixture stirred at room temperature for ten minutes. The mixture was stirred for 20 minutes with an excess of 2N NaOH in MeOH and concentrated to dryness. It was then acidified to pH 3 with HCl and extracted with EtOAc. The organic phase was concentrated in vacuo and purified by preparative HPLC to yield the title compound (isomer b; 30 mg). LCMS (ESI): calc. C25H25ClFN5O4=513; obs. M+H=514.3. Retention time: 2.24 min. [0467] LC/MS Method: flow rate: 1.5 mL/min; Buffer A: 0.1% TFA/H2O; Buffer B 0.1% TFA/MeCN; gradient elution from 5-100% B over 3.6 minutes, then 100% B for 1.0 minute, detection at 254 nm.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; THERAVANCE BIOPHARMA R&D IP, LLC; Fleury, Melissa; Beausoliel, Anne-Marie; Hughes, Adam D.; Long, Daniel D.; Wilton, Donna A.A.; US2015/209352; (2015); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

These common heterocyclic compound, 1001401-62-2, name is 2-(2H-1,2,3-Triazol-2-yl)benzoic acid, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Recommanded Product: 1001401-62-2

To a solution of 2-(2H-1,2,3-triazol-2-yl)benzoic acid (500 mg, 2.65 mmol) in DMF (8 mL) was added HATU (1.51 g, 3.98 mmol) and DIEA (1.03 mg, 7.95 mmol). The resulting mixture was stirred at RT for 30 mins, and then tert-butyl hexahydropyrrolo[3,4-cjpyrrole- 2(1H)-carboxylate (562 mg, 2.65 mmol) was added. The resulting mixture was stirred at RT for2 h. The reaction mixture was filtered and the filtrate was concentrated in vacuo. The residue was purified by silica gel column chromatography (10% – 50% EtOAc in petroleum ether) to give the title compound as a oil. LRMS m/z (M+H) 384.2 found, 384.2 required.

The synthetic route of 2-(2H-1,2,3-Triazol-2-yl)benzoic acid has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK SHARP & DOHME CORP.; KUDUK, Scott, D.; LIVERTON, Nigel; REGER, Thomas, S.; SKUDLAREK, Jason, W.; (50 pag.)WO2016/100162; (2016); A2;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 7170-01-6, name is 3-Methyl-1H-1,2,4-triazole, A new synthetic method of this compound is introduced below., HPLC of Formula: C3H5N3

4-Fluoro-2-(3-methyl-1H-1,2,4-triazol-1-yl)benzonitrile and 4-fluoro-2-(5-methyl-1H-1,2,4-triazol-1-yl)benzonitrile. A solution of 2,4-difluorobenzonitrile (7.07 g, 50.8 mmol) and 3-methyl-1H-1,2,4-triazole (4.22 g, 50.8 mmol) in N,N-dimethylformamide (45 ml) was treated with powdered anhydrous potassium carbonate (10 g) and the resulting mixture was stirred at 22 C. for 18 h. The solid was then filtered and the filtrate was concentrated in vacuo. The residue was diluted with ethyl acetate, washed with water and brine, dried over anhydrous magnesium sulfate and concentrated. The mixture containing the 2 and 4-triazolyl-benzonitriles was purified by a combination of chromatography on silica gel (elution gradient of ethyl acetate in hexane) and on reversed phase silica gel to give 1.86 g (18% yield) of Intermediate 64 and 0.526 g (5% yield) of Intermediate 65. 4-Fluoro-2-(3-methyl-1H-1,2,4-triazol-1-yl)benzonitrile. white crystals (ethyl acetate-hexane); mp 117-118 C. 1HNMR 400 MHz (CDCl3) delta (ppm): 2.54 (3H, s, CH3), 7.24 (1H, m, CH), 7.62 (1H, dd, J=2.5 Hz and J=9.1 Hz, CH), 7.84 (1H, dd, J=5.6 Hz and J=8.6 Hz, CH), 8.82 (1H, s, CH). Anal. Calcd for C10H7FN4: C 59.40, H 3.49, N 27.71; Found: C, 59.25; H, 3.32; N, 27.81. 4-fluoro-2-(5-methyl-1H-1,2,4-triazol-1-yl)benzonitrile. white crystals (ethyl acetate-hexane); mp 120-121 C. 1HNMR 400 MHz (CDCl3) delta (ppm): 2.56 (3H, s, CH3), 7.30 (1H, dd, J=2.5 Hz and J=8.1 Hz, CH), 7.39 (1H, m, CH), 7.91 (1H, dd, J=5.5 Hz and J=8.6 Hz, CH), 8.06 (1H, s, CH). Anal. Calcd for C10H7FN4: C 59.40, H 3.49, N 27.71; Found: C, 59.35; H, 3.70; N, 27.77.

The synthetic route of 7170-01-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Naidu, B. Narasimhulu; US2005/256109; (2005); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics